Applied Nanoscience (2022) 12:4019–4032

https://doi.org/10.1007/s13204-022-02634-z

ORIGINAL ARTICLE

Characterization and photocatalytic activity of ­TiO2 nanoparticles

on cotton fabrics, for antibacterial masks
Marco Antonio Alvarez‑Amparán1   · Vanessa Martínez‑Cornejo1   · Luis Cedeño‑Caero1   ·
Kevin A. Hernandez‑Hernandez2,3   · Rubén D. Cadena‑Nava2   · Gabriel Alonso‑Núñez2   ·
Sergio Fuentes Moyado2 

Received: 28 June 2022 / Accepted: 30 August 2022 / Published online: 15 September 2022
© King Abdulaziz City for Science and Technology 2022

Abstract
The in-situ impregnation of two commercial cotton fabrics (lab coat and Indiolino) with ­TiO2 nanoparticles ­(TiO2-NPs) was
carried out. For this, two commercial cotton fabrics were dipped in titanium isopropoxide, titanium butoxide and titanium
tetrachloride solutions to the ­TiO2-NPs formation and in-situ ­TiO2-NPs impregnation on the cotton fabric surface by the
sonochemical, hydrothermal and solvothermal methods, respectively. The impregnated fabrics were characterized by ATR-
FTIR, SEM–EDS, Raman, UV–Vis, DRS and tension tests. The results showed the successful formation and impregnation
of ­TiO2-NPs on both cotton fabrics. The leaching of ­TiO2-NPs from cotton fabrics was negligible after several washing
cycles. The self-cleaning properties and antibacterial activity of ­TiO2-NPs functionalized cotton fabrics were assessed by
photocatalytic and antibacterial tests. The photocatalytic activity was determined by the degradation of methylene blue dye
under UV and solar irradiation. The materials showed good photoactivity, since MB was degraded up to 99% under solar
and UV irradiations in 60 min. The bactericidal capacity of the ­TiO2-NPs on fabrics, evaluated in-situ by SEM, showed that
Indiolino presented the best antibacterial properties against Escherichia coli and Bacillus pumilus.

Keywords  Titania nanoparticles · Antibacterial masks · Cotton fabrics · Sonochemical synthesis · Hydrothermal synthesis

Introduction pandemic caused by the SARS-CoV-2 virus has potentiated

The development of fabrics with antibacterial and antiviral
activity and self-cleaning properties has been triggered in
the last decades due to healthcare industry and home tex-
tiles applications (Hussain 2020; Yocupicio-Gaxiola et al.
2021; Konda et al. 2020; Botequim et al. 2012; Montazer
and Seifollahzadeh 2011). Moreover, the current COVID-19
* Marco Antonio Alvarez‑Amparán
malvarez@quimica.unam.mx
* Luis Cedeño‑Caero
caero@unam.mx
1
UNICAT, Departmento de Ingeniería Química, Facultad
de Química, Universidad Nacional Autónoma de México,
04510 Ciudad de Mexico, México
2
Centro de Nanociencias y Nanotecnología (CNyN‑UNAM),
Universidad Nacional Autónoma de México,
22800 Ensenada, Baja California, México
3
Centro de Investigación Científica y de Educación Superior
de Ensenada (CICESE), Ensenada, Baja California, México
the exhaustive research on this type of functionalized fabrics
since these ones could help avoiding the virus dispersion
(Yocupicio-Gaxiola et al. 2021; Militky et al. 2021). The
cotton fabrics are the main textile used in the healthcare
industry since the cotton surface could be electrostatically
charged, in an analogous way as on the natural silk surface
(Konda et al. 2020). In this sense, since the cotton fabric is
a porous and hydrophilic material, antibacterial agents can
be added over the cotton surface. Also, the addition of an
antiviral agent to the textile fibers is an interesting option as
additional protection to avoid virus infections for both the
wearer and those around them.
The selection of an antiviral agent should be based on
its antiviral activity, level of toxicity, method of applica-
tion and cost. Also, antiviral agents added to textile fibers
must be active even in the presence of a wide class of
microorganisms, stable, durable, safer for the user and not
harmful to the environment. It has been shown that inor-
ganic nanoparticles (NPs) can inactivate virus due to the
viral envelope rupture by the generation of oxidant species

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(Botequim et al. 2012; Ogunsona et al. 2020, Yaqoob et
al. 2020). Also, it is important to mention that inorganic
NPs may act as adsorbents, catalysts or photocatalysts,
which could enhance or promote high antibacterial activ-
ity. Currently, inorganic NPs and their composites are
a viable alternative to manufacture multifunctional and
antiviral fibers (Hussain 2020; Yocupicio-Gaxiola et al.
2021). Among others inorganic NPs, ­TiO2 nanoparticles
­( TiO 2 -NPs) have attracted attention because they are
biocompatible, non-toxic, and inexpensive (Yocupicio-
Gaxiola et al. 2021). The incorporation of T ­ iO2-NPs on
textile fibers provides them with antiviral properties, UV
protection, promotes surface hydrophobicity/hydrophilic-
ity, could act as flame retardant, and provide self-cleaning
properties (Hussain 2020; Yocupicio-Gaxiola et al. 2021;
Montazer and Seifollahzadeh 2011, Lessan et al. 2011;
Senić et al. 2011). The antibacterial activity of T­ iO2-NPs
is attributed to the fact that they can produce reactive oxy-
gen species (ROS) in the presence of UV irradiation, since
­TiO2-NPs is a semiconductor material, acting as a photo-
catalyst. Also, ­TiO2-NPs antibacterial activity has been
observed in dark conditions, however, the action mecha-
nism is not yet fully understood (Ogunsona et al. 2020).
The synthesis of T ­ iO2-NPs by sonochemical irradia-
tion at low temperatures has been reported as an efficient
method to obtain nanocrystals of suitable size (Guo et al.
2003). In a similar sense, Prasad et al. (2010) reported the
synthesis of T­ iO2-NPs by the sol–gel method assisted by
ultrasound at low temperature. Additionally, the impregna-
tion of several types of NPs on the surface of cotton fibers
by ultrasonic irradiation has been reported previously, e.g.,
Ag nanoparticles (Hadad et al. 2007), ZnO nanoparticles
(Perelshtein et al. 2009a), CuO nanoparticles (Perelshtein
et  al. 2009b) and T ­ iO 2-NPs (Perelshtein et  al. 2012).
Akhavan et al. (2014) and Montazer and Seifollahzadeh
(2011) have reported the immobilization of ­TiO2-NPs on
cotton using the ultrasound-assisted sol–gel method, obtain-
ing the anatase phase without requiring subsequent heating.
Complementary, cotton fabrics impregnated with ­TiO2-NPs
by ultrasound showed high resistance to the leaching under
several washing cycles, maintaining their self-cleaning, anti-
bacterial, and antiviral properties (Akhavan et al. 2014).
In this work, to obtain fabrics with antibacterial prop-
erties, cotton fabrics with ­TiO2-NPS were synthetized by
several methods. Cotton fabrics were analyzed by ATR-
FTIR, Raman and SEM–EDS to assess the appropriate
formation and impregnation of the ­TiO2-NPs on the sur-
face of the fibers. Photocatalytic degradation of methylene
blue (MB) was carried out under UV and solar irradiation
to assess the self-cleaning properties. The MB degrada-
tion rate was discussed in terms of the pseudo-first order
kinetic constants. Escherichia coli and Bacillus pumi-
lus bacteria were incubated on the functionalized cotton
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Applied Nanoscience (2022) 12:4019–4032
fabrics and were exposed to solar and UV irradiation to
corroborate the antibacterial properties of the synthetized
materials.
Materials and methods
Materials
Commercial lab coat (100% cotton, 244 g/m2) and Indi-
olino (100% cotton, 175 g/m2) fabrics were used as model
textiles. Titanium isopropoxide ­(C12H28O4Ti, 98%), glacial
acetic acid (­ CH3COOH, 98%), titanium chloride (­ TiCl4,
98%) and titanium butoxide (Ti(OBu) 4, 98%) were pro-
vided by Sigma-Aldrich and used without further puri-
fication. Before the treatments, the fabrics were washed
with a non-ionic detergent and dried for 24 h at 70 °C.
All impregnation procedures were carried out using
5 cm × 5 cm of cotton squares.
Synthesis and incorporation of TiO2‑NPs on cotton
fabrics
Modified cotton fabrics were obtained from three synthesis
methods of T­ iO2-NPs, in each one the preparation method
was improved varying the synthesis parameters, such as:
loading of Ti precursor, treatment and synthesis temperature,
reaction time and washing conditions.
Sonochemical synthesis
The ­TiO2-NPs impregnation on cotton fibers by sonochemi-
cal synthesis was carried out according to the methodol-
ogy proposed by Akhavan et al. (2014) and Montazer and
Seifollahzadeh (2011) and it was adapted according to our
purposes. Briefly, the ­TiO2 nanocrystals were synthesized
and simultaneously impregnated on cotton fabrics under
ultrasonic irradiation by hydrolysis of titanium isopropox-
ide (IPT) in the presence of distilled water, using acetic
acid as hydrolysis catalyst. In a typical preparation, distilled
water and glacial acetic acid were placed in a flask, then the
solution was stirred for 5 min at room temperature (RT).
Subsequently, a 5 × 5 cm of cotton piece was immersed into
the solution and the flask was placed in an ultrasonic bath
(Brason 2200; 50 kHz, 220 W) for 5 min at RT. Afterwards,
1 mL of IPT was added dropwise to the solution in the bath
and the temperature was increased to 65 °C and kept con-
stant for 4 h. After the reaction time, the flask was removed
from the ultrasound bath and the cotton squares were dried
Applied Nanoscience (2022) 12:4019–4032 4021

at RT in a desiccator for 24 h. The fabrics were washed with
distilled water and dried at 70 °C for 24 h.
Hydrothermal synthesis
The cotton samples were first dried at 70  °C for 4  h to
remove adsorbed water and immediately dipped for 12 h
into a 1 wt.% solution of titanium butoxide (BuOT) in a
mixture of tertbutanol and acetic acid (90/10 wt.%). Sam-
ples were then removed and dried at 60 °C for 2 h in an
oven, to evaporate the solvent, and then transferred into a
200 mL Teflon-lined stainless steel autoclave, half-full of
water, which was then placed in an oven maintained at the
required temperature (i.e. 110 °C) for the hydrothermal treat-
ment during 3 h. Finally, samples were dried at 50 °C for 2 h
(Abid et al. 2016).
Solvothermal synthesis
The procedure for the synthesis of T­ iO2 nanomaterials (Wu
et al. 2007) was adapted to obtain NPs-TiO2 on the cotton
samples by solvothermal method as follows, a certain vol-
ume of T ­ iCl4 (1.0–9.0 mL) was quickly dropped into a fixed
volume of acetone (60 mL) under vigorous stirring at RT.
The obtained solution and cotton fabrics were transferred to
a Teflon-lined autoclave and sealed. The autoclave was then
placed in an oven for solvothermal treatment at 100 °C for
12 h. After cooling at RT, the cotton fabrics were removed,
washed several times with acetone and finally dried at 50 °C
for 2 h.
The nomenclature used for the synthesized materials is
shown in Table 1, where commercial fabrics were labeled
according to the cotton fabric (I or C for Indiolino or Cot-
ton lab coat, respectively), Ti precursor (I, B and T for IPT,
BuOT or Ti chlorine, respectively) and the method used
(U, S or H; for sonosynthesis (ultrasound), solvothermal
or hydrotreated method, respectively). The synthesis tem-
perature, the reaction time and the Ti loading (for selected
samples, with best performance) are included as reference
in Table 1.
Photocatalytic tests
Methylene blue degradation tests using UV radiation
The photocatalytic properties of the T­ iO2-NPs functional-
ized cotton samples were analyzed based on the methylene
blue (MB) degradation, which was previously impregnated
on the surface of the cotton fabrics. The cotton samples
were cut into 2.5 cm × 2.5 cm squares and were impregnated
with a MB solution (3 mL, 5 ppm). Then, the fabrics were
exposed to UV-light source (320 nm) with an intensity of
3.5 mW/cm2. The MB degradation was followed by UV–Vis
DRS of the fabric squares at 0, 15, 30, 60 and 120 min of
UV-light exposure. The maximum absorbance value ­(C0)
was determined by UV–Vis DRS spectroscopy. Meanwhile,
the UV–Vis DRS absorption spectra of the fabrics contain-
ing MB were obtained at 0, 15, 30, 60 and 120 min of UV-
light exposure. The rate of dye decomposition was calcu-
lated and compared based on the C/C0 values, where ­C0 and
C represent the initial MB concentration on the impregnated
cotton pieces and the MB concentration at the time t, respec-
tively (Pakdel and Daoud 2013).
Methylene blue degradation tests using solar
radiation
The photocatalytic degradation of MB using ­TiO2-NPs
functionalized cotton fabrics were also assessed using solar
irradiation, in similar procedure to UV irradiation, before
described. In this case, the cotton samples were placed in a
container and then exposed to sunlight. The average natural
day light irradiation intensity was 4 mW/cm2, in winter from
9 am to 3 pm in Mexico City.
Antibacterial tests
Cell culture
For the bactericidal tests of the fabrics impregnated with
­TiO2-NPs, Escherichia coli (MC4100) and Bacillus pumilus
(B-41243) strains were used, which are gram-negative and
gram-positive bacteria, respectively. Escherichia coli is a

Table 1  Nomenclature of the Fabric Method Precursor Time (h) Temperature Ti (wt.%)*

synthesized materials (°C)

IIU Indiolino Sonosynthesis IPT 4 65 2.7

IBH Indiolino Hydrothermal BuOT 3 110 2.8
CIU Cotton lab coat Sonosynthesis IPT 4 65 2.6
CBH Cotton lab coat Hydrothermal BuOT 3 110 2.4
CTS Cotton lab coat Solvothermal TiCl4 12 100 n.d
*
 Evaluated by SEM–EDS

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gram-negative bacterium, rod shaped (2.0–6.0 µm in length)
bacteria with rounded ends (Conti and Gettner 1962; Per-
cival et al. 2014). Bacillus pumilus is a gram-positive bac-
terium, rod shaped (0.5–10 μm length) bacteria (Borsa et al.
2016; Grutsch et al. 2018). A freshly bacterial culture was
prepared for each of the bacteria to study the bacterial activ-
ity of the samples. From an overnight culture of E. coli and
B. pumilus, 900 μL were taken and added to 45 mL of fresh
LB medium. Then the bacterial mediums were incubated
using a New Brunswick Scientific G-25 Incubator Shaker,
at 150 rpm and 37 °C, until their optical density reached 0.1
at 600 nm ­(OD600 = 0.1). The optical density of the bacte-
rial culture was measured using a Thermo Multiskan GO
spectrophotometer at 600 nm.
Bactericidal activity of TiO2‑NPs on fabrics
To study the bacterial activity, 4 μL of fresh bacteria culture
was placed on squares fabrics of 0.5 × 0.5 cm. Then, the
fabric pieces inoculated with bacteria were exposed to UV
radiation (254 nm) using an Air Science UV-Box decontami-
nation chamber. The fabrics were irradiated with UV light
(254 nm) for 2.5 and 5 min on both sides. Subsequently, the
cloth samples were incubated in petri dishes with LB agar
for 18 h at 37 °C to study antibacterial activity.
Bactericidal in‑situ study by SEM
After the samples were incubated, the antibacterial activity
was analyzed by SEM Hitachi SU3500. The samples were
dried at RT and placed on a sample holder using carbon
tape. Then, the samples were analyzed at low vacuum condi-
tions (25 Pa) and 7 kV. The images were taken at different
magnifications (47X, 270X, 370X, 2000X and 3000X) and
recorded digitally.
Washing tests
The cotton pieces were subjected to several washing cycles
to determine the leaching of the ­TiO2-NPs. The washing
cycles were carried out according to the textile standard
FZ/T 73,023–2006 as follow: the cotton fabrics impreg-
nated with T
­ iO2-NPs were immersed in an ultrasound device
(100 Hz) at 40 °C for 5 min. The washed cotton fabrics were
removed and rinsed with distilled water. Afterwards, the cot-
ton pieces and the washing water were analyzed by UV–Vis
DRS and UV–Vis spectroscopy (respectively) to determine
the amount of ­TiO2-NPs leached (Akhavan et al. 2014).
Characterization
Attenuated total reflectance infrared spectroscopy (ATR-
FTIR) was carried out in Nicolet 6700 FTIR spectrometer
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Applied Nanoscience (2022) 12:4019–4032
to corroborate the formation and successfully impregnation
of ­TiO2-NPs on the cotton fabrics. Raman spectroscopy and
DxR Raman microscope Thermo Scientific was used to cor-
roborate the surface characteristics of the materials. The syn-
thesis solutions and the water from the washing tests were
analyzed by UV–Vis spectroscopy at RT (Varian Cary 50)
from 200 to 1100 nm to assess the impregnated Ti amount
and the leached Ti amount, respectively. Scanning electron
microscopy (SEM) coupled to energy dispersive spectros-
copy (EDS) system was carried out using a Jeol JSM-5900
LV microscope to the morphological and elemental analysis.
Surface area of cotton samples was determined using N ­ 2
adsorption–desorption isotherms at – 196 °C on a Tristar
Micrometrics apparatus; the samples were degassed 8 h in
vacuum at 350 °C. Tensile strength of the samples chemi-
cally treated and without treatment were tested on a Digital
traction force Gauge, LZKW. The MB degradation on the
surface of the cotton pieces was analyzed by UV–Vis diffuse
reflectance spectroscopy (UV–Vis DRS) by a Perkin Elmer
Lambda 365.
Results and discussion
SEM–EDS micrographs and elemental mapping
All fabrics were analyzed by SEM–EDS. It is important to
note that to obtain nano size particles, an optimum Ti load-
ing should be immobilized on the cotton fabrics so as not
to lose Ti species in the washing process by leaching. The
cotton fabrics shown in Table 1 have an optimum Ti loading
and, therefore only the highest Ti loading samples showed
SEM–EDS signal due to the sensibility of the technique.
Since those nano particles would only be observed appropri-
ately by the TEM. Therefore, the SEM technique helped to
select the optimum Ti loading corresponding to NPs domain
(reported in Table 1).
Figure 1 shows the micrographs and elemental mapping
of selected impregnated cotton fabrics. Figure 1a corre-
sponds to the impregnated lab coat fabrics by sonochemical
method (CIU) at 100X resolution. From Fig. 1a can be sug-
gested the correct synthesis method since the observed size
of ­TiO2 corresponds to the NPs domain. Figure 1b shows
the micrograph at 1000X resolution and it can be observed
that the cotton threads are covered by ­TiO2-NPs (white dots)
with an adequate particle size distribution on the cotton sur-
face as it was also observed in Fig. 1a. Figure 1c shows the
micrograph of cotton fabric without supported ­TiO2-NPs.
Figure 1d shows the elemental mapping of Ti, confirming
the adequate Ti distribution on the cotton fabric. For com-
parison purposes, Fig. 1e and 1f show a sample with high
Ti loading than the cotton fabric shown in Fig. 1a and 1b.
Both micrographs shown the microparticles domain of these
Applied Nanoscience (2022) 12:4019–4032 4023

Fig. 1  Micrographs and elemental mapping of CIU (a–d) and fabrics with high Ti loading (e and f)

samples with high Ti loading. Similar results (no shown)
were obtained for all fabrics.
Tensile and textural properties of fabrics
The Table 2 shows the surface area determined by ­N2 phys-
isorption, the lattice thread diameter, the grammage and the
tensile strength of the cotton fabrics. The tensile strength of
the fabrics was assessed using the bare cotton fabrics and
after a first and a second treatments. The surface area of
the cotton fabrics is too low, less than 1 ­m2g−1, which is a
typical value for cotton fabrics. Also, due to this low value
of surface area, the immobilization of the T ­ iO2-NPs should
be carried out in a proper way to avoid T ­ iO2-NPs leaching

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Table 2  Tensile properties of the cotton fabrics
Surface area Lattice thread Grammage
­(m2/g) diameter (mm) (g/m2)
Indiolino 0.4 0.38 175
Lab coat 0.6 0.30 244
a
 1st treatment: ultrasound for 2 h and dried for 24 h at 65 °C
b
 2nd treatment: ultrasound for 5 h and dried for 24 h at 110 °C
due to the saturation of OH- surface groups on the cotton
fabrics. According to the previous SEM–EDS results, the
morphological characteristics suggested that T ­ iO2-NPs was
successfully synthetized and as will be seen later, the immo-
bilization of ­TiO2-NPs was carried out satisfactorily.
The lattice thread diameter of lab coat and Indiolino is
very similar, the difference is only 0.08 mm, which indi-
cates the great similarity of both cotton-derived fabrics.
Also, this feature explains in great manner the low value of
surface area since the cotton fabrics are made up of inter-
twined threads. Additionally, the thin structure of the cot-
ton fabrics threads emphasizes that their surface can only
be coated by very small structures such as nanoclusters or
nanoparticles. The grammage represents the cotton fabric
weight per unit area and as it can be observed, its value is
greater for the lab coat cotton than for Indiolino. The gram-
mage value difference is due to the density values that are
slightly different due to the final preparation of the fabrics.
Therefore, it could be inferred that lab coat cotton fabrics
present a greater interaction with ­TiO2-NPs on their surface.
The tensile strength of the cotton fabrics, without and with
ultrasound treatments, is an important characteristic since
the immobilization of T ­ iO2-NPs could largely depend on
this property. That is, in addition to the fact that T
­ iO2-NPs
immobilization on the cotton fabrics surface is a function of
physisorption and to the chemisorption phenomena, prob-
ably ­TiO2-NPs interaction with OH- surface groups could
also be influenced by the mechanical stability of the inter-
twined threads of cotton fabrics. Breaking loads of Indiolino
and Lab coat fabrics were 9.90 and 8.33 N, respectively.
After first treatment (the immersion of cotton fabrics in an
ultrasound bath for 2 h and then a drying process at 65 °C),
the fabrics were about 54 and 25% more resistant than
the pristine one. The acidic condition of reaction solution
(pH = 3.5) and ultrasonic irradiation did not cause destruc-
tion on the structure of cotton. After the second treatment
(the cotton fabrics were maintained for 5 h under ultrasound
irradiation and finally a dried process at 110 °C), the fabrics
were about 10% less resistant than fabrics with only one
first treatment but were more resistant than untreated fabrics.
This loss on tensile strength fabric could be related to the
ultrasonic irradiation and/or cleavage of the cellulosic chains
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Applied Nanoscience (2022) 12:4019–4032
Tensile strength of bare Tensile strength after 1st Tensile strength
cotton fabrics (N) treatment (N)a after 2nd treatment
(N)b
9.90 15.22 13.82
8.33 10.39 9.21
by acid hydrolysis (Akhavan et al. 2014). In addition, shrink-
age might occur while sonication causing a slight increase
in breaking elongation from 5 to 6%. The results indicated
that in-situ sonosynthesis of T ­ iO2-NPs on the cotton fabric
did not cause any significant damage to on the structure of
cotton, as has also been stated by Akhavan et al. (2014).
In contrast, the fabric prepared by solvothermal method
(CTS) from T ­ iCl4 at 100 °C in the autoclave produces HCl.
Therefore, strong acidic condition of reaction solution pro-
vokes the destruction of the structure of cotton. Even neu-
tralizing the acid conditions, was not possible to preserve
the structure of cotton and this preparation method was
discarded.
Raman spectroscopy
Cotton fibers are composed of the biopolymer β-cellulose
(Fig.  2), whose repeating units are β-D-glucose mol-
ecules and are linked by β-1,4-glucoside bonds (Pakdel
and Daoud et al. 2013). Its fibers have a great amount of
hydroxyl groups on the cellulose surface, so that extensive
research have been made about the chemical functionaliza-
tion of this material taking advantage of this high reactive
functional group (OH-). The reactivity of cotton is a func-
tion of the considerable number of hydroxyl groups located
on the C2, C3 and C6 carbons in each β-D-glupiranose or
anhydroglucose unit (Pakdel and Daoud 2013; Al-Taweel
and Saud 2016).
Al-Taweel and Saud  (2016) stated that the ­TiO2-NPs
can interact strongly with surface hydroxyl and carboxyl
groups of cotton cellulose. Additionally, Pakdel and Daoud
Fig. 2  β-D-glucose molecules
Applied Nanoscience (2022) 12:4019–4032 4025
(2013), Daoud and Xin (2004) and Daoud et al. (2005) pro-
pose an anchoring mechanism for T ­ iO2/SiO2 composites on
the cotton surface where nanoparticles are anchored on the
hydroxyl groups of the C2, C3 and C6 carbons in cellulose.
Therefore, it can be suggested that T
­ iO2-NPs synthetized and
immobilized by ultrasonic irradiation as in this work, could
be anchored on the surface of cotton fabrics in a similar way
as commented above. In this sense, the Fig. 3 shows the
Raman spectra of Degussa P25, IIU and CIU. From Fig. 3a it
can be observed the strong absorption at 151 ­cm−1 (Eg) cor-
responding to the vibrational mode of anatase T ­ iO2 NPs and
less intense bands at 398 ­cm−1 (B1g o A1g and B1g), also
for this phase. The bands at 514 ­cm−1 (Eg) and 643 ­cm−1
(A1g) are assigned to rutile phase of TiO2, according to
Qina et al. (2009), Burlacov et al. (2006) and Hana et al.
(2018). The observed red shift for the bands is because the
increase of critalinity of the sample and, also could be by the
interaction of anatase and rutile ­TiO2 phases.
The observed bands at 1094, 578, 516, 433 and
383 ­cm−1 for CIU (Fig. 3c) corresponding at vibrational
modes of cellulose. According with Abid et al. (2017),
the most intense band at 1094 ­c m −1 could be assigned
to the C–O–C symmetric and assymetric stretching mode
of the glycosidic bonds of the celulose`s glucopyranose
ring. Figure 3c shows the vibrational modes at 144, 151,
383, 516, 513 and 638 ­c m −1, which are characteristics
to ­TiO2-anatase nanoparticles, in agree accordance with
Fig. 3  Raman spectra of a
Ti Degussa P25, b Indiolino
prepared by ultrasound irradia-
tion (IIU) and c cotton lab coat
prepared by ultrasound irradia-
tion (CIU)
published literature (Al-Taweel and Saud 2016). These
bands are assigned to the extension of the Ti–O bond (Eg)
at 639 ­cm−1, the bending of the Ti–O bond (A1g + B1g)
at 517 ­cm−1 and the bending of the O-Ti–O bond (Eg) at
397 ­cm−1. It can be observed a red shift in the Eg mode
frequencies for the T ­ iO2-NPs supported on the cotton fab-
rics, i.e., the band at 151 ­cm−1 for the supported ­TiO2-NPs
(see Fig. 3c) correspond to the red shift of the band at
145 ­cm−1 for ­TiO2-anatase nanoparticles.
According to Abid et al. (2017), the red shift could be
attributed to the phonon confinement effect due to the
minor size of the T ­ iO2-NPs and the crystallinity increase.
Even, the interaction between ­TiO2-NPs and -OH groups
on the cotton fabric could contributed to this effect. For
Indiolino prepared by ultrasound irradiation (IIU) (Fig. 3b)
it can be observed an intense band at 152 ­cm−1 and less
intense bands at 650 ­cm−1, 1741  ­cm−1, 2913  ­cm−1. The
first two bands could be related to anatase ­TiO2-NPs and
the bands at 1741 ­cm−1, 2913 ­cm−1 could be assigned to
the characteristic vibrational modes of cellulose and T ­ iO2
phases. As for CIU, the red shift in the IIU Raman spec-
trum can be explained by the minor size of the T ­ iO2-NPs
and/or the interaction between surface -OH groups of cot-
ton fabrics and ­TiO2-NPs. From these results, for both IIU
and CIU, the presence of T ­ iO2-NPs intense bands allows
to suggest the adequate functionalization of the cotton
fabrics.
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4026 Applied Nanoscience (2022) 12:4019–4032

alone does not show the increasing absorption band below

800 ­cm−1, which allowed to corroborate that this region can
be attributed to the presence of ­TiO2-NPs.

UV–Vis spectra of reaction and washing solutions

Figure 5 shows the UV–Vis spectra of the preparation and

washing solutions of the synthetized fabrics. T ­ iO2 spectrum
presents an absortion band at ~ 270—280 nm and therefore
it is possible the identification of the T
­ iO2-NPs in the prep-
aration and washing effluents (Akhavan et al. 2014). It is
important to note that ­TiO2-NPs physically adsorbed on the
fabric surface are likely to leach into the washing solution.
The spectrum of CIU prepared with an excess of IPT and the
CIU prepared with an adequately amount of IPT are shown
in Fig. 5 (a and b, respectively). The CIU prepared with
an excess of IPT showed the greatest absorbance of the all
Fig. 4  FTIR-ATR spectra of: a cotton fabric, b CIU without washing, analized samples. The UV–Vis spectrum of CIU prepared
and c CIU after 5 washing cycles with an adequately amount of IPT shown an absortion band
around of ~ 270—280 nm, which is less intense than the
sample with an excess of IPT. CBH, IBH and IIU samples
Attenuated total reflectance infrared spectroscopy showed even lower values of absortion. Also, the UV–Vis
(FTIR‑ATR) analysis of subsequent washing solutions showed no absorp-
tion bands suggesting that the ­TiO2-NPs do not leach from
Figure 4 shows the FTIR-ATR spectra of the cotton lab coat the fabric surface. The above results indicated that the good
fabric and CIU. The bands at 1161 and 1030 ­cm−1 corre- immobilization of ­TiO2-NPs on the cotton fibers.
spond to the tension vibration of the functional groups C–C It is important to mention that ­TiO 2-NPs could be
and C-O of cellulose, respectively. For all samples, a broad anchored on hydroxyl and/or carboxyl groups by covalent
band between 3336 and 3280 ­cm−1 is observed, which is linkages (Akhavan et al. 2014). The chemically anchored
characteristic of O–H functional groups in cellulose (Ugur ­TiO2-NPs on the hydroxyl and carboxyl groups of the cotton
et al. 2010). surface must be the preponderant species that persist after
These bands, characteristic of cellulose and observed in
cotton fabric, persistent in CIU without and with washing
treatment showing that the textile was not modified appre-
ciably. Only was observed to shift of these bands to high
wavelengths values, it could be attributed to the interaction
of ­TiO2-NPs to cotton surface.
From 800  ­cm−1 toward longer wavelength, it can be
observed the evolution of a broad region. According to
Praveen et al. (2014) the region from 1000 ­cm−1 to 400 ­cm−1
correspond to the Ti–O stretching and Ti–O-Ti bridging
stretching modes of the T ­ iO2-NPs. Also, it is reported that
around 450 ­cm−1 presents absorption band which is attrib-
uted to the ­TiO2 NPs. The lack of definition in Fig. 4 below
800 ­cm−1 is due to FTIR-ATR was carried out with a dia-
mond crystal with a range 4000–550 ­cm−1, which does not
allow a good definition of this region. However, the obtained
results allow to establish the presence of ­TiO2-NPs (crystal-
line ­TiO2-anatase phase) on the cotton fabric surface. Fig-
ure 4 shows the FTIR-ATR spectra of the CIU before and
after washing processes (Fig. 4b-c). As reference, the spec-
Fig. 5  UV–Vis spectra of washing effluents: a CIU prepared with
trum of the alone cotton fabric is shown (Fig. 4a). It can be excess of IPT, b CIU, c CBH, d IBH, e IIU andf water solution as
observed that the FTIR-ATR spectrum of the cotton fabric reference

13
Applied Nanoscience (2022) 12:4019–4032 4027
the washing tests, in agreement with Akhavan et al. (2014)
and Montazer and Seifollahzadeh (2011).
According to Ugur et al. (2010), the simultaneous synthe-
sis of T
­ iO2-NPs and the functionalization of cotton fibers in
a one-step process by sonochemical irradiation can be rep-
resented by a hydrolysis reaction (Eq. 1) and a condensation
reaction (Eq. 2) as follow:
(1)
( )
Ti OC3 H7 4 + H2 O → (Ti − OH)n + C3 H7 OH
(Ti − OH)n → (Ti − O − Ti)m + H2 O
The formation of T ­ iO2-NPs can be explained in two steps
as follow: 1) The hydrolytic Ti species, formed by the IPT
hydrolysis in water, are condensed in many gel nuclei units
and then are aggregated in large clusters. 2) The ·OH and ·H
radicals, formed by the water sonolysis due to the cavitation
process by the ultrasound irradiation, promote the hydrolysis
of IPT and the polycondensation of Ti–OH groups, generat-
ing the T
­ iO2-NPs. According to Ugur et al. (2010), the sono-
chemical formation of ­TiO2-NPs is carried out in the liquid
phase, around the collapsing bubble and not within the col-
lapsing cavity. The ­TiO2-NPs generation is a function of the
microturbulence and the shock waves. The microturbulence
is due to the radial liquid movement by the cavitation of the
bubbles. The shock waves are a result of the high-pressure
waves emitted by collapsing bubbles. The conjunction of
microturbulence and the shock waves phenomena generates
a localized heat and pressure transient zones. Large tempera-
ture and pressure gradients cause water sonolysis, therefore
·OH and ·H radicals are generated and promoting the Ti–OH
condensation. It is proposed that nucleation ratio increases
Fig. 6  MB degradation on IBH samples under solar irradiation (b to e; at 15, 30, 60 and 120 min, respectively) and under UV irradiation (g to j;
at 15, 30, 60 and 120 min, respectively). a bare IBH and f IBH impregnated with MB solution
by the shock waves and the growth rate of the nanocrystals
is a function of the microturbulence.
Photocatalytic activity
The photocatalytic activity of the ­TiO2-NPs on cotton fabrics
was assessed to corroborate the self-cleaning properties and
the antiviral and antibacterial features. Since as it has been
established the ROS generation is a key factor. In this sense,
the photocatalytic degradation of model molecules such as
(2) dyes has been carried out as elsewhere (Hosseini‑Sarvari
et  al. 2022; Skiba and Vorobyova  2020). In this sense,
5 × 5 cm squares of the fabrics were impregnated with MB
(methylene blue) solution (10 ppm) and subsequently irradi-
ated with UV (320 nm) or solar irradiation. The adsorbed
amount of MB did not exceed 5% for all cotton samples,
which is indicative of the low adsorption capacity of the
material, due mainly to the low surface area of the materi-
als (see Table 2). Due to the characteristic blue color of the
Indiolino cotton fabric it was not possible to determine the
MB degradation by DRS. For this reason, white color cotton
indiolino was used for the photodegradation tests. Prior to
irradiation, the 5 × 5 cm squares were cut off in four parts
(2.5 × 2.5 cm) and were placed in a set-up in such a way that
all samples were irradiated with the same intensity. Further,
the set-up was stored in the darkness for 1 h to discard any
possible change in the concentration, resulting from the pho-
tolysis process (Abid et al. 2016). Figure 6 shows the MB
degradation on IBH under solar (Fig. 6b to 6e) and under
UV irradiation (Fig. 6g to 6j). It can be observed a notice-
able decrease of the blue color on the cotton fabrics after UV
and solar irradiation. The discoloration observed was due
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4028
to the photocatalytic degradation of MB by the T ­ iO2-NPs
presence, showing the efficiency of the functionalized cot-
ton fabrics.
Also, the changes of the MB concentration on the fabrics
were determined by UV–Vis DRS absorption at 0, 15, 30,
60 and 120 min of light exposure. According to Uddin et al.
(2007), the observed band at 664 nm is assigned at dimeric
and trimeric MB species adsorbed on the surface. The MB
degradation was determined as the total MB conversion, by
the C/C0 relationship. Figure 7 shows the MB degradation,
using IBH under UV irradiation in the photoreactor. It can
be observed that MB was degraded almost 70% in 60 min.
It is important to mention that the MB degradation of CIU
(not shown) was near to 99% in 60 min under UV irradia-
tion. Also, it was observed negligible change in the MB con-
centration in the presence of bare cotton fabric under UV
or solar irradiation, which confirmed the effective role of
the ­TiO2-NPs in the photocatalytic activity. Based on these
results it is possible to infer that IPT is a better option as Ti
precursor than BuOT.
The MB degradation data were well fitted with a pseudo-
first order kinetics. Table 3 shows the kinetic results of MB
degradation using the lab coat and Indiolino fabrics pre-
pared by sonochemical or hydrothermal methods. Under UV
irradiation, for the fabrics synthesized by different method
and Ti precursor, it can be observed that pseudo-first order
kinetic constants for Indiolino fabrics (IBH and IIU) are
higher than for the cotton fabrics (CBH and CIU); 0.01
vs. 0.0067/min and 0.0117 vs. 0.0075 ­cm−1 (respectively).
Fig. 7  DRS results of MB degradation on IBH, obtained by UV irra-
diation
Table 3  Kinetic results of MB photo degradation of NPs-TiO2 on cotton fabrics by solar light (sun) or UV irradiation (uv)
CIU sun CIU uv CBH sun
K ­(min−1) 0.0165 0.0075 0.0154
13
Applied Nanoscience (2022) 12:4019–4032
Meanwhile, the pseudo-first order kinetic constants under
solar irradiation are higher for Lab coat than Indiolino fab-
rics. The kinetic constants are: 0.0165 for CIU vs. 0.0142 for
IIU and 0.0154 for CBH vs. 0.0117 for IBH.
The higher pseudo-first order kinetic constants values for
Indiolino fabrics compared with cotton fabrics, under UV
irradiation, probably could be because the lightly longer size
of ­TiO2 crystals for Indiolino fabrics, since as it has been
stated the ­TiO2 particles of larger size are more photoactive
under shorter wavelengths, UV spectrum (Senić et al. 2011;
Uddin et al. 2007). Contrarily, the higher photoactivity for
cotton fabrics, under solar irradiation, it can be explained
by two effects or by the combination of both. The first one
could be due to the shorter size of T ­ iO2 crystals for cotton
fabrics which could absorb longer wavelength photons, in
visible spectrum. The second one could be due to the greater
amount of the irradiated photons under solar irradiation.
Figure 8 shows the MB degradation using CIU under sun-
light irradiation. It can be observed that almost a complete
MB degradation was achieved in 120 min. Additionally, the
Table 3 show that the pseudo-first order kinetic constant
for CIU under solar irradiation was higher than pseudo-first
order kinetic constants for IBH and IIU (1.4 and 1.2 times,
respectively). The aforementioned results confirmed the
higher photoactivity of functionalized cotton lab coat fab-
rics compared to the functionalized Indiolino fabrics under
solar irradiation.
Fig. 8  DRS results of MB degradation on CIU, obtained by sunlight
irradiation
CBH uv IBH sun IBH uv IIU sun IIU uv
0.0067 0.0117 0.0100 0.0142 0.0117
Applied Nanoscience (2022) 12:4019–4032 4029
Fig. 9  Characteristic degradation time (τ) of MB for all synthetized
cotton fabrics under UV or solar (sun) irradiation
The characteristic degradation time (τ) is the time needed
to degrade half of the contaminant species present in the
experiment. Figure 9 shows the τ of MB under UV or solar
irradiations. For all samples (CIU, CBH, IBH and IBU), τ
was reached faster under solar irradiation than under UV
irradiation. That is, the same cotton fabric (cotton lab coat
or Indiolino) prepared by the same method and Ti precur-
sor and used under solar irradiation showed a greater MB
degradation than when UV radiation was used on the same
fabrics. These results are according to the reported pseudo-
first order kinetic constants in Table 3 discussed earlier.
This behavior could be due to the simultaneous effect of the
shorter size of T
­ iO2 crystals for cotton fabrics (which absorb
visible irradiation) and the greater amount of the irradiated
photons under solar irradiation. In general, the functional-
ized cotton samples synthetized in this work shown an ade-
quately structure and a successful photocatalytic behavior as
has been discussed previously.
Bactericidal activity of ­TiO2‑NPs on fabrics
The bactericidal activity of the fabrics synthesized was not
possible to study by Kirby-Bauer technique because these
ones do not form inhibition region, which has also been pre-
viously reported with fabrics impregnated with ­TiO2-NPs
(Singhal et al. 2021). For this reason, fabrics squares of
0.5 cm × 0.5 cm from IIU, IBH, CIU and CBH were inocu-
lated with the E. coli bacteria and were evaluated in Petri
dishes with LB-agar medium. After the inoculation without
UV irradiation, it was found that the IIU sample, ­TiO2-NPs
impregnated Indiolino fabric by sonosynthesis and using iso-
propoxide as Ti precursor, has a greater capacity to inhibit
E. coli, (see Fig. 10, sample 1). Also, CIU showed good
antibacterial capacity (sample 3). The fabrics prepared by
hydrothermal method, IBH (sample 2) and CBH (sample
Fig. 10  Antibacterial activity of the fabrics on petri dish LB-agar.
Sample 1: IIU, sample 2: IBH, sample 3: CIU, sample 4: CBH. Con-
trols samples (5 and 6) correspond to cotton lab coat and Indiolino,
respectively
4), showed the shorter bacterial inhibition capacity. It is
important to note that Indiolino without T ­ iO2-NPs (sample
6) showed bactericidal capacity, in a minor amount of its
counterparts that contain ­TiO2-NPs. The halo of bacteria
around the Indiolino fabric in sample 6 is more homogene-
ous than the other ­TiO2-NPs treated fabrics.
Based on the bactericidal results obtained in the Petri
dishes, the in-situ antimicrobial activity analysis was car-
ried out by SEM only for IIU sample and its corresponding
control. The E. coli and B. pumilus bacteria was grown on
the surface of the Indiolino fabric (control sample), which
can be observed in the SEM micrographs in Fig. 11a and
Fig. 11c. In both cases it was possible to observe the bac-
teria at 2000X magnification (see Fig. 11b y 11d and it can
be observed that the bacteria cover most of the Indiolino
surface. The E. coli (Fig. 11b) and B. pumilus (Fig. 11d)
bacteria show no apparent damage, and it is observed a
normal morphology and size, in agree with (Percival et al.
2014; Grutsch et al. 2018). In the case of T­ iO2-NPs treated
Indiolino fabric, the bactericidal activity was significantly
appreciated by means of SEM, see Fig.  12. Fig  12a, b
show the fabrics at low magnification (1300X) where the
homogeneous deposition of the T ­ iO2 and bacteria can be
observed. In Figure b and Figure d, the bacteria E. coli
and B. pumilus can be seen in greater detail (see insets).
In both cases, the areas without T ­ iO 2-NPs showed the
presence of bacteria, that is the bacteria grew in zones
without ­TiO2 deposits, which demonstrates the ability to
inhibit both bacteria. When the samples are irradiated with
UV irradiation for 2.5 min on both sides, it is possible to
observe a greater bactericidal capacity on the fabric sur-
face, see Fig. 13. The Fig. 13a shows the E. coli biofilm
with abnormal morphology or damage. From Fig. 13b it
can be observed that bacteria only grew on areas without
NPs, as was analyzed for the other Indiolino fabrics. In the
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4030 Applied Nanoscience (2022) 12:4019–4032

Fig. 11  SEM micrographs of
Indiolino fabric inoculated with
E. coli (a) and B. pumilus (c).
Micrographs at 2000X magni-
fication for E. coli (b) and B.
pumilus (d)

Fig. 12  SEM micrographs at
1300X of T ­ iO2-NPs treated
Indiolino fabric and inoculated
with E. coli (a) and B. pumilus
(c). Micrographs at high mag-
nification (> 1300X) for E. coli
(b) and B. pumilus (d)

case of the fabric inoculated with B. pumilus, the bacteria
were totally eliminated (see Fig. 13c) under UV irradia-
tion. Additionally, bacteria were not found on the fabric
surface, even the areas without NPs are free of bacillus.
When the Indolino fabrics were exposed for 5 min on both
sides, both bacteria were no longer found in the fabric with
and without ­TiO2-NPs.
The IIU sample showed the best bactericidal capacity,
which could be due to a better distribution of the NPs on
Indiolino surface when the sonosynthesis method is used.

13
Applied Nanoscience (2022) 12:4019–4032 4031
Fig. 13  SEM micrographs of treated ­TiO2-NPs Indiolino fabric under UV irradiation for 2.5 min on both sides (5 min total), inoculated with E.
coli (a) and B. pumilus (c). Micrograph magnifications of E. coli (b) and B. pumilus (d) on the Indiolino fabric
According to the in-situ SEM analysis, the better the nano-
particles are distributed, the greater the antimicrobial effect
that results. Therefore, the homogeneity of the T­ iO2-NPs on
the surface fabric should be considered to have an efficient
bactericidal capacity.
Conclusions
Titania nanoparticles ­(TiO2-NPs) were successfully syn-
thesized and simultaneously immobilized on cotton fab-
rics by several methods. The synthesis of T ­ iO2 anatase and
its impregnation was confirmed by UV–Vis, SEM–EDX,
Raman and FTIR-ATR spectroscopy.
The leaching of the ­TiO2-NPs from the cotton fabrics
after washing cycles was analyzed by UV–Vis and the char-
acteristic band of anatase ­TiO2-NPs was observed at a very
low intensity suggesting the adequate impregnation of the
­TiO2-NPs on the cotton fibers.
The ­TiO2-NPs functionalized cotton fabrics degraded
99% of methylene blue in 60 min by photocatalysis under
UV and solar irradiation confirming self-cleaning properties.
The bactericidal capacity of the impregnated T ­ iO2-NPs,
determined by in-situ SEM analysis, against E. coli (gram
negative) and B. pumilus (gram positive) was greater for
Indiolino cotton. The T ­ iO2-NPs homogeneous distribution
on the cotton fabric surface enhance the bactericidal capac-
ity which is favored by the sonosynthesis method using Ti
isopropoxide as precursor.
The results show that, it is feasible the functionalization
of cotton fabrics with photoactive ­TiO2-NPs to produce face
masks with good bactericidal capacity and self-cleaning
properties.
Acknowledgements  We thank to H. Fabián Alonso-Cordero (UMAC-
CICESE) for the SEM analysis, and Iván Puente (FQ-UNAM) for the
SEM-EDS analysis.
Author contributions  Conceptualization: SFM, LCC; LCC, Formal
análisis: GAN, RDCN, SFM; Funding acquisition: SFM, LCC; Inves-
tigation: LCC, VMC, RDCN, KAHH; Methodology: LCC, VMC,
RDCN, KAHH; Project administration: SFM; Resources: SFM;
Supervision: SFM; Validation: MAAA; Visualization: MAAA; Roles/
Writing—original draft: MAAA; Writing—review & editing: MAAA.
Funding  This work was funded by the Dirección General de Asun-
tos del Personal Académico (DGAPA) of the Universidad Nacional
Autónoma de México (UNAM) by the Research Support Program
(PAPIIT, project IV100121).
Declarations 
Conflict of interest  On behalf of all authors, the corresponding author
states that there is no confict of interest.
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